CN112843109A - Method for removing nicotine and triazole pesticide residues in total saponins of stems and leaves of saponin plant - Google Patents
Method for removing nicotine and triazole pesticide residues in total saponins of stems and leaves of saponin plant Download PDFInfo
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- CN112843109A CN112843109A CN201911100795.2A CN201911100795A CN112843109A CN 112843109 A CN112843109 A CN 112843109A CN 201911100795 A CN201911100795 A CN 201911100795A CN 112843109 A CN112843109 A CN 112843109A
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- saponin
- leaves
- eluting
- water
- stems
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- 229930182490 saponin Natural products 0.000 title claims abstract description 65
- 235000017709 saponins Nutrition 0.000 title claims abstract description 65
- 150000007949 saponins Chemical class 0.000 title claims abstract description 61
- 239000001397 quillaja saponaria molina bark Substances 0.000 title claims abstract description 44
- 239000000447 pesticide residue Substances 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 27
- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 title claims abstract description 24
- 229960002715 nicotine Drugs 0.000 title claims abstract description 24
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 150000003852 triazoles Chemical class 0.000 title claims abstract description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 109
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 49
- 239000011347 resin Substances 0.000 claims abstract description 32
- 229920005989 resin Polymers 0.000 claims abstract description 32
- 238000000605 extraction Methods 0.000 claims abstract description 28
- 239000000706 filtrate Substances 0.000 claims abstract description 20
- 239000002904 solvent Substances 0.000 claims abstract description 18
- 239000000047 product Substances 0.000 claims abstract description 17
- 239000012535 impurity Substances 0.000 claims abstract description 14
- 239000000284 extract Substances 0.000 claims abstract description 13
- 238000001914 filtration Methods 0.000 claims abstract description 13
- 239000010410 layer Substances 0.000 claims abstract description 13
- 238000002360 preparation method Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 8
- 239000003960 organic solvent Substances 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 6
- 239000012044 organic layer Substances 0.000 claims abstract description 5
- 238000010298 pulverizing process Methods 0.000 claims abstract description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 12
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 9
- 239000003814 drug Substances 0.000 claims description 5
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 4
- 238000010828 elution Methods 0.000 claims description 4
- 206010028980 Neoplasm Diseases 0.000 claims description 3
- 239000008280 blood Substances 0.000 claims description 2
- 210000004369 blood Anatomy 0.000 claims description 2
- 230000036772 blood pressure Effects 0.000 claims description 2
- 230000008569 process Effects 0.000 claims description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M sodium bicarbonate Substances [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims 2
- 208000024172 Cardiovascular disease Diseases 0.000 claims 1
- 230000032683 aging Effects 0.000 claims 1
- 239000012141 concentrate Substances 0.000 claims 1
- 230000002708 enhancing effect Effects 0.000 claims 1
- 230000036039 immunity Effects 0.000 claims 1
- 229910000029 sodium carbonate Inorganic materials 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 30
- 239000000575 pesticide Substances 0.000 abstract description 12
- 229930182494 ginsenoside Natural products 0.000 abstract description 6
- 229940089161 ginsenoside Drugs 0.000 abstract description 6
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 30
- 235000003140 Panax quinquefolius Nutrition 0.000 description 23
- 239000000243 solution Substances 0.000 description 23
- 244000131316 Panax pseudoginseng Species 0.000 description 22
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 18
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 18
- 235000008434 ginseng Nutrition 0.000 description 18
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 16
- 241000196324 Embryophyta Species 0.000 description 15
- 239000012071 phase Substances 0.000 description 11
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- 230000000844 anti-bacterial effect Effects 0.000 description 6
- 239000003899 bactericide agent Substances 0.000 description 6
- 238000001514 detection method Methods 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 238000001179 sorption measurement Methods 0.000 description 6
- 239000011550 stock solution Substances 0.000 description 6
- 240000005373 Panax quinquefolius Species 0.000 description 5
- 238000007865 diluting Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 239000005906 Imidacloprid Substances 0.000 description 4
- 235000003181 Panax pseudoginseng Nutrition 0.000 description 4
- 239000005941 Thiamethoxam Substances 0.000 description 4
- 239000005846 Triadimenol Substances 0.000 description 4
- 239000003480 eluent Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000005457 ice water Substances 0.000 description 4
- YWTYJOPNNQFBPC-UHFFFAOYSA-N imidacloprid Chemical compound [O-][N+](=O)\N=C1/NCCN1CC1=CC=C(Cl)N=C1 YWTYJOPNNQFBPC-UHFFFAOYSA-N 0.000 description 4
- 229940056881 imidacloprid Drugs 0.000 description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 4
- -1 panaxadiol saponins Chemical class 0.000 description 4
- 239000011780 sodium chloride Substances 0.000 description 4
- NWWZPOKUUAIXIW-FLIBITNWSA-N thiamethoxam Chemical compound [O-][N+](=O)\N=C/1N(C)COCN\1CC1=CN=C(Cl)S1 NWWZPOKUUAIXIW-FLIBITNWSA-N 0.000 description 4
- BAZVSMNPJJMILC-UHFFFAOYSA-N triadimenol Chemical compound C1=NC=NN1C(C(O)C(C)(C)C)OC1=CC=C(Cl)C=C1 BAZVSMNPJJMILC-UHFFFAOYSA-N 0.000 description 4
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 3
- SYFJYASKXNAXKC-UHFFFAOYSA-N Panaxadiol Natural products CC1(C)CCCC(O1)C2CCC3(C)C2C(O)CC4C5(C)CCC(O)C(C)(C)C5CCC34C SYFJYASKXNAXKC-UHFFFAOYSA-N 0.000 description 3
- 239000005821 Propamocarb Substances 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 235000020710 ginseng extract Nutrition 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000007935 neutral effect Effects 0.000 description 3
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 3
- WZZLDXDUQPOXNW-UHFFFAOYSA-N propamocarb Chemical compound CCCOC(=O)NCCCN(C)C WZZLDXDUQPOXNW-UHFFFAOYSA-N 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- WURBVZBTWMNKQT-UHFFFAOYSA-N 1-(4-chlorophenoxy)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)butan-2-one Chemical compound C1=NC=NN1C(C(=O)C(C)(C)C)OC1=CC=C(Cl)C=C1 WURBVZBTWMNKQT-UHFFFAOYSA-N 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 241000180649 Panax notoginseng Species 0.000 description 2
- 235000003143 Panax notoginseng Nutrition 0.000 description 2
- 229960000583 acetic acid Drugs 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- 239000012490 blank solution Substances 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000003085 diluting agent Substances 0.000 description 2
- FBOUIAKEJMZPQG-BLXFFLACSA-N diniconazole-M Chemical compound C1=NC=NN1/C([C@H](O)C(C)(C)C)=C/C1=CC=C(Cl)C=C1Cl FBOUIAKEJMZPQG-BLXFFLACSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 235000019253 formic acid Nutrition 0.000 description 2
- 239000012362 glacial acetic acid Substances 0.000 description 2
- 235000013402 health food Nutrition 0.000 description 2
- 239000012046 mixed solvent Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- HWPKGOGLCKPRLZ-UHFFFAOYSA-M monosodium citrate Chemical compound [Na+].OC(=O)CC(O)(C([O-])=O)CC(O)=O HWPKGOGLCKPRLZ-UHFFFAOYSA-M 0.000 description 2
- 235000018342 monosodium citrate Nutrition 0.000 description 2
- 239000002524 monosodium citrate Substances 0.000 description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000013558 reference substance Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- 239000001509 sodium citrate Substances 0.000 description 2
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 2
- 235000011083 sodium citrates Nutrition 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 241000607479 Yersinia pestis Species 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000000132 electrospray ionisation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002481 ethanol extraction Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- 150000002215 flavonoids Chemical class 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- 239000004009 herbicide Substances 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000002917 insecticide Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000001294 liquid chromatography-tandem mass spectrometry Methods 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000002414 normal-phase solid-phase extraction Methods 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 230000001766 physiological effect Effects 0.000 description 1
- 239000000419 plant extract Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000001953 sensory effect Effects 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 235000002639 sodium chloride Nutrition 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 239000003206 sterilizing agent Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
- 239000000341 volatile oil Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/25—Araliaceae (Ginseng family), e.g. ivy, aralia, schefflera or tetrapanax
- A61K36/258—Panax (ginseng)
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P25/00—Drugs for disorders of the nervous system
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P3/00—Drugs for disorders of the metabolism
- A61P3/06—Antihyperlipidemics
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61P35/00—Antineoplastic agents
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- A61P37/02—Immunomodulators
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- A61P39/00—General protective or antinoxious agents
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- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
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- A61P39/06—Free radical scavengers or antioxidants
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P9/00—Drugs for disorders of the cardiovascular system
- A61P9/12—Antihypertensives
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation or decoction
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
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Abstract
The invention relates to a preparation method for extracting low-pesticide residue ginsenoside from saponin plant stems and leaves, which takes the saponin plant stems and leaves as raw materials, and comprises the following steps: (1) pulverizing saponin plant stems and leaves, adding extraction solvent for extraction, adjusting pH of the extract, and filtering to obtain filtrate; (2) adsorbing the filtrate with macroporous resin column, removing impurities with eluting solvent, washing, discarding, eluting with aqueous ethanol, concentrating the eluate to a certain volume, extracting with organic solvent, discarding the organic layer, adsorbing the water layer with macroporous resin column, eluting with 80-95% ethanol, discarding the eluate, concentrating the lower column solution, and drying to obtain corresponding stem leaf total saponin product. The content of the total saponins prepared by the method is more than 80 percent, and the residue of nicotine and triazole pesticides is less than 0.01 ppm.
Description
Technical Field
The invention relates to the field of medicinal plant extracts, in particular to a method for removing nicotine and triazole pesticide residues in total saponins of stems and leaves of saponin plants.
Background
The saponin plant stems and leaves such as ginseng stems and leaves, American ginseng stems and leaves, and pseudo-ginseng stems and leaves contain various effective components such as saponins, flavonoids, volatile oils and the like, wherein the saponins are substances with the most obvious physiological activity and have pharmacological activities in various aspects such as tumor resistance, cancer resistance, blood pressure reduction, blood fat reduction, fatigue resistance and the like. In recent years, a large number of reports about saponin preparation processes of ginseng stems and leaves, American ginseng stems and leaves and pseudo-ginseng stems and leaves are relatively mature, but the raw materials are easily damaged by pests due to the growth characteristics of the raw materials, a large number of insecticides, sterilizing agents, herbicides and the like need to be sprayed in the planting process, and the pesticide spraying area of plant stems and leaves contacting pesticides is large and is a part with more pesticide residues, so that the quality of the stem and leaf raw materials is greatly influenced by the use of the pesticides. At present, saponin products using stems and leaves as raw materials often have more pesticide residues, and nicotine and triazole bactericides among the saponin products are several kinds of pesticides with larger residual quantity, and the pesticide residues reduce the quality of the products and seriously reduce the competitiveness of naturally extracted saponin products in the international market, so the problem of the pesticide residues of the saponin extracts using the stems and leaves as the raw materials needs to be solved urgently.
The prior art CN103550273A discloses a method for extracting low-pesticide residue ginsenoside from ginseng, which comprises the steps of leaching ginseng with cold water, concentrating, extracting with a solvent, and eluting with macroporous resin to obtain a low-pesticide residue ginsenoside extract. In the technical scheme, the pesticide residue does not contain nicotine and triazole pesticides with large pesticide residue in stem and leaf plants.
The prior art CN106581108A discloses a method for removing pesticide propamocarb in a ginseng extract, which is to extract by a mixed solvent of petroleum ether and ethyl acetate, then filter by a mixture of LX-N1, LX-N2 type macroporous resin and 40-60 mesh neutral alumina, and the recovery rate of ginsenoside after the treatment is 80-85%, and the propamocarb is less than 0.01 ppm. The technical scheme only aims at the removal of propamocarb pesticide, and does not relate to the nicotine and triazole pesticides described in the application.
The prior art CN1765917A discloses a method for extracting panaxadiol saponins, which comprises the steps of cutting ginseng or American ginseng, adopting 60-98% ethanol for cold extraction, decompressing and concentrating an extracting solution, adding water for adjusting the pH value to 9-10, then putting an alkaline concentrated solution on macroporous resin, eluting with water and then 70% ethanol to obtain total saponins, further recovering ethanol from an obtained eluent containing the total saponins, and using n-butyl alcohol for extracting the panaxadiol saponins. The concentration of the eluent used in the last macroporous resin separation step in the preparation method of the technical scheme is different from that of the invention, and further extraction, separation and purification steps and secondary macroporous resin adsorption are lacked, so that the technical problem of removing pesticide residues is not solved.
In the prior art, most of the raw materials for extracting saponin are rhizome parts of ginseng, pseudo-ginseng and the like, the parts are traditional Chinese medicinal material medicine parts, the cost for extracting the saponin components is high, the stem and leaf components are rarely used as medicines in the traditional Chinese medicine preparation and do not belong to traditional medicine parts, and the saponin plant stem and leaf parts are selected as the extraction raw materials, so that the utilization rate of the saponin-containing plant resources is improved.
Due to the difference of the application parts and the update of pesticides, the prior art lacks a targeted research on an extraction method for reducing nicotine and triazole pesticide residues in saponin obtained by plant extraction. The technical scheme fills the blank in the field, and provides a method for simply, conveniently and efficiently removing nicotine and triazole pesticide residues in total saponins of saponin plant stems and leaves.
Disclosure of Invention
The invention aims to solve the technical problem that saponin plant stems and leaves are used as raw materials to extract low nicotine, such as imidacloprid, thiamethoxam and the like; triazole, such as triadimenol, diniconazole, etc. The method has the advantages of good effect of removing pesticide residue in the ginseng stem and leaf, American ginseng stem and leaf, and panax notoginseng stem and leaf total saponin products, easy operation, low cost, and high content of effective components in the prepared products.
The technical scheme adopted by the invention for solving the technical problems is as follows: a method for removing nicotine and triazole pesticide residues in total saponins of stems and leaves of saponins plants sequentially comprises the following steps:
(1) pulverizing saponin plant stems and leaves, adding extraction solvent, extracting, adjusting the pH of the extractive solution to alkalinity, and filtering to obtain filtrate.
(2) Adsorbing the filtrate with macroporous resin column, removing impurities with eluting solvent, washing, discarding, eluting with aqueous ethanol, concentrating the eluate to a certain volume, extracting with organic solvent, discarding the organic layer, adsorbing the water layer with macroporous resin column, eluting with 95% ethanol, discarding the eluate, concentrating the lower column solution, and drying to obtain corresponding total saponin product.
The crushing mesh number of the saponin plant stems and leaves in the step (1) is 14 meshes to 80 meshes.
The extraction solvent in the step (1) is water or hydrous ethanol, and preferably 50-80% of hydrous ethanol.
When the alkalinity is adjusted in the step (1), any alkaline agent can be used, and KOH and Na are preferred2CO3、NaHCO3And one or more of NaOH.
The model of the macroporous resin used in the impurity removal of the filtrate in the step (2) can be any model of macroporous adsorption resin column, and the preferred model of the macroporous resin is D101, D101C, AB-8, LSA-12 and D941.
In the step (2), the eluting solvent used for removing impurities is water and hydrous ethanol, and the eluting solvent is water and then 15-35% hydrous ethanol. The volume of the elution concentrated solution is 1/5-1/10 of the volume of the raw material solution.
In the step (2), the organic solvent extraction is any organic solvent with low polarity, preferably one or more of dichloromethane, chloroform, ethyl acetate or n-hexane.
In the step (2), when the water layer of the extract is purified by using macroporous resin, any type of macroporous adsorption resin column can be used, and the types of the macroporous resin are preferably D101, D101C, AB-8 and LXPR-2.
The preferable technical scheme of the application comprises the following steps:
(1) taking saponin plant stems and leaves, crushing the stems and leaves into 14-80 meshes, adding a water or aqueous ethanol extraction solvent, adjusting the pH value of an extract to 8-13, and filtering to obtain a filtrate.
(2) Adsorbing the filtrate with macroporous resin column, eluting with water to eliminate impurity, eluting with 20-35% concentration water containing alcohol to eliminate impurity, and eluting with 60-80% concentration water containing alcohol. Concentrating the eluate to a certain volume, extracting with organic solvent, removing organic layer, adsorbing the water layer with macroporous resin column, eluting with 80-95% ethanol, removing eluate, concentrating and drying the eluate to obtain corresponding total saponin product.
According to the technical scheme, various nicotine and triazole pesticide components in the stems and leaves of the saponin plants can be effectively removed through the adjustment of the pH value of the extracting solution, the extraction with the organic solvent and the second macroporous resin separation, so that the pesticide residue in the product is less than 0.01 ppm.
The total saponin extracts prepared by the method have extremely low nicotine and triazole pesticide residues, high saponin content, simple and easy operation and low cost.
Detailed Description
The present invention will be described in further detail with reference to examples and comparative examples below:
the determination method of ginsenoside content in the examples and comparative tests refers to the item "twenty-three, determination of total saponins in health food" in the 2003 edition "inspection and evaluation of health food technical Specifications". The determination method comprises the following steps: precisely absorbing 50 mu l of a sample, placing the sample in a test tube with a plug, placing the test tube in a water bath to volatilize a solvent, adding 0.2mL of 5% vanillin-glacial acetic acid solution and 0.8mL of perchloric acid, uniformly mixing, fully dissolving residues, heating the mixture in the water bath at 60 ℃ for 15min, taking out the mixture, immediately placing the mixture in the ice water bath to cool for 10min, adding 5.0mL of glacial acetic acid, shaking up the mixture, taking a corresponding reagent as a blank solution, and immediately measuring the absorbance value of the blank solution at the wavelength of 560nm of an ultraviolet-visible spectrophotometer.
The pesticide residues in the examples and the comparative tests are determined by the following method, and the total amount of the nicotine pesticide residue and the triazole pesticide residue is the sum of the contents of the measured components.
Nicotine (imidacloprid and thiamethoxam)
Instruments and materials
1. The main instrument, high performance liquid chromatography Agilent1260, is provided with an ultraviolet detector, a chromatographic column model C18, a 4.6mm × 25cm, 5 μm ultrasonic extractor, a digital display temperature control water bath kettle and a homogenizer. 2. And (3) standard substance: imidacloprid and thiamethoxam standard substance provided by scientific research and monitoring of environmental protection in the rural area. 3. Reagent: acetonitrile, chromatographic purity. Methanol, pure chromatography. Sodium chloride, guaranteed purity. A solid phase extraction column and an amino column with the volume of 6mL are filled with 500 mg. Filter, 0.2 μm, organic series.
(II) test procedure
Preparation of a reference substance: 0.01g of 2 bactericide standards (accurate to 0.0001g) are weighed into different 10mL volumetric flasks respectively, diluted with acetone to a constant volume to prepare 1.0mg/mL standard stock solutions. Respectively transferring 1.0mL of 2 standard stock solutions of single bactericides (imidacloprid and thiamethoxam) into the same 100mL volumetric flask, and diluting with acetonitrile to a constant volume to be calibrated. A mixed standard stock solution (10. mu.g/mL) was prepared.
Sample preparation: weighing 5.00g of sample in a 250mL beaker, adding 50.0mL of acetonitrile, homogenizing in a high-speed homogenizer (15000r/min) for 2min, filtering by using filter paper to a 100mL stoppered measuring cylinder (containing 6g of sodium chloride), collecting filtrate, covering a measuring cylinder plug, violently shaking for 1min, discharging gas in the measuring cylinder during shaking, and finally standing at room temperature for more than 30min to separate the acetonitrile phase and the water phase.
Purification 10.00mL of the acetonitrile phase solution was aspirated from the cylinder, charged into a 100mL beaker, placed on a 70 ℃ water bath (with ventilation), acetonitrile was evaporated, and 2.0mL of methanol + dichloromethane (5+95) was added to dissolve the residue as it dried, and further purification was awaited. The amino column was pre-washed with 5.0mL of methanol + dichloromethane (5+95) eluent, the solution to be purified was immediately added when the solvent level was close to the amino column adsorption layer, collected in a 50mL beaker, the beaker containing the residual solution was rinsed with 4mL of methanol + dichloromethane (5+95) eluent, passed through the column, and repeated once. Heating the beaker in a 50 deg.C water bath, evaporating to almost dry, adding methanol + water (1+1) to 5mL for several times, filtering with 0.2 μm organic filter membrane, and detecting.
Detection conditions are as follows: wavelength 270nm, mobile phase methanol/water (1: 1, V/V), flow rate 1.0mL/min, injection amount 25 μ L, detection time 15 min.
Bis-or triazoles (triadimenol, diniconazole)
Instruments and materials
An API4000 quadrupole tandem mass spectrometer (ABI, USA) equipped with an electrospray ionization source (ESI); 1200 series high performance liquid chromatograph (Agilent corporation, usa); sigma3-30K centrifuge (Sigma, Germany); VX200 vortex shaker (Labnet, USA); LE612-L electronic balance (sensory: 0.01g, Sidolis instruments, Germany). 2.2 bactericide standards of triadimenol and triadimefon; 3. reagent: acetonitrile, formic acid (chromatographically pure, TEDIA corporation, usa); anhydrous magnesium sulfate, sodium chloride, sodium citrate, sodium dihydrogen citrate, PSA adsorbent (chromato-pure, agilent, usa); the water is ultrapure water.
(II) Experimental procedure
Preparation of a reference substance: 0.01g of 2 bactericide standards (accurate to 0.0001g) are weighed into different 10mL volumetric flasks respectively, diluted with acetone to a constant volume to prepare 1.0mg/mL standard stock solutions. Respectively transferring 1.0mL of 2 standard stock solutions of single bactericides (triadimenol and triadimefon) into the same 100mL volumetric flask, and diluting with acetonitrile to a constant volume to be calibrated. A mixed standard stock solution (10. mu.g/mL) was prepared.
Sample preparation: weigh 2g of sample (exactly 0.01g) into a 50mL covered centrifuge tube, add 10mL of water, and shake until the sample is sufficiently wetted with water. Standing for 10min, transferring 10mL of acetonitrile into a centrifuge tube, adding 50 μ L of internal standard solution, and placing the centrifuge tube on a vortex mixing and shaking instrument to shake for 1min at the speed of 2000 r/min. The centrifuge tube was kept at 0 ℃ for 10min, then 4g of anhydrous magnesium sulfate and 1g of sodium chloride, 1g of sodium citrate and 0.5g of sodium dihydrogen citrate were added to the centrifuge tube, immediately shaken on a vortex mixer shaker at 2000r/min for 2min and then centrifuged at 4000r/min for 10 min.
1mL of the supernatant was transferred to a 1.5mL centrifuge tube, 150mg of anhydrous magnesium sulfate and 25mg of PSA adsorbent were added, the mixture was shaken on a vortex mixer shaker at 2000r/min for 2min, and centrifuged at 6000r/min for 2 min. The supernatant was aspirated and filtered through a 0.45 μm organic phase filter, 200 μ L was pipetted, diluted to 1mL with acetonitrile and detected by LC-MS/MS.
The detection conditions are as follows:
a chromatographic column: AtiantisdC18(150 mm. times.2.1 mm, 3 μm); mobile phase: acetonitrile-0.1% aqueous formic acid (volume fraction), flow rate: 0.2 mL/min; column temperature: 30 ℃; sample introduction amount: 10 μ L.
Mass spectrum scanning mode: scanning positive ions; electrospray ion source (ESI); flow rate of atomizing gas: 414 kPa; air flow of the air curtain: 69 kPa; auxiliary heating air flow: 414 kPa; ionization temperature: 500 ℃; collision gas flow rate: 69 kPa; the 4 gases are all nitrogen; residence time: 30 ms; ionization voltage: 5500V, positive ion MRM mode acquisition.
Example 1
Taking 100g of ginseng stem and leaf raw materials, crushing, sieving with a 14-mesh sieve, adding water with the pH of 9, and decocting for 2 times, wherein the first dosage is 16 times of the raw materials and is decocted for 2 hours, and the second dosage is 16 times of the raw materials and is decocted for 1.5 hours. Mixing decoctions, adjusting pH to 9 with NaOH solution, filtering, adsorbing the filtrate with D101 macroporous resin, adsorbing, eluting with 3 times column volume of water for removing impurities, eluting with 3 times column volume of 35% ethanol for removing impurities, eluting with 3 times column volume of 60% ethanol, concentrating the 60% ethanol eluate until no alcohol smell exists, diluting with water to 100ml, extracting with n-hexane, discarding n-hexane layer, adsorbing the water layer with macroporous resin column, adsorbing with macroporous resin column, desorbing with 95% ethanol, discarding the eluate, concentrating and drying the lower column solution to obtain total saponin of caulis Et folium Ginseng with content of 85.4%, and total content of nicotine and triazole pesticide residue of 0.006 ppm.
Example 2
100g of American ginseng stem and leaf raw material is taken, crushed and sieved by a 14-mesh sieve, 70 percent of aqueous ethanol is adjusted to pH value of 9, the pH value is added into the raw material for extraction for 4 times, the first dosage is 6 times of the raw material, and the other three dosages are 4 times of the raw material. Mixing the extractive solutions, adjusting pH to 9 with KOH solution, filtering, adsorbing the filtrate with D101C macroporous resin, adsorbing, eluting with 3 times column volume of water for removing impurities, eluting with 3 times column volume of 30% ethanol for removing impurities, eluting with 3 times column volume of 70% ethanol, concentrating 70% ethanol eluate until no alcohol smell exists, diluting with water to 100ml, extracting with dichloromethane and n-hexane, discarding the organic layer, adsorbing the water layer with macroporous resin column, adsorbing with adsorption column, eluting with 85% ethanol, discarding the eluate, concentrating and drying the lower column solution to obtain total saponin product of stem leaf of radix Panacis Quinquefolii with content of 84.5%, and total content of nicotine and triazole pesticide residue of 0.006 ppm.
Example 3
100g of the stem and leaf raw materials of the pseudo-ginseng are taken, crushed and sieved by a 14-mesh sieve, added with water with the pH value of 11 and decocted for 2 times, the first time is 16 times of the raw materials and decocted for 2 hours, and the second time is 16 times of the raw materials and decocted for 1.5 hours. Mixing decoctions, adjusting pH to 10 with KOH solution, filtering, adsorbing the filtrate with D101 macroporous resin, eluting with 3 times column volume of water to remove impurities, eluting with 3 times column volume of 35% ethanol to remove impurities, eluting with 3 times column volume of 60% ethanol, concentrating the 60% ethanol eluate until no alcohol smell exists, diluting with water to 100ml, extracting with dichloromethane, discarding dichloromethane, adsorbing the water layer with macroporous resin column, eluting with 80% ethanol, discarding the eluate, concentrating and drying the lower column solution to obtain Notoginseng radix stem and leaf total saponin product. The content is 82.3 percent, and the total amount of the nicotine pesticide residue and the triazole pesticide residue is 0.005 ppm.
And (3) comparison test:
comparative example 1: extracting the ginseng stems and leaves by adopting an extraction method recorded in CN 106581108A:
1) taking 100g of ginseng stem and leaf raw material, crushing the raw material into 40-60 meshes, placing the raw material into a round-bottom flask, adding 700mL of water, heating, timing from boiling, extracting for 3 hours, filtering, and collecting feed liquid; adding 500mL of water into filter residue, heating, timing from boiling, extracting for 2 hours, filtering, collecting feed liquid, combining the two extracted feed liquids, and concentrating under vacuum at 60 ℃ to obtain 150mL of ginseng extract;
2) using petroleum ether in volume ratio: ethyl acetate ═ 1: 1.5, extracting the ginseng extract for 10 times at the normal temperature by using the mixed solvent with the same volume, and taking the lower-layer feed liquid;
3) adding 50g of a mixture of LX-N1, LX-N2 type macroporous resin and 40-60 mesh neutral alumina (the mass ratio of LX-N1 to LX-N2 type macroporous resin to 40-60 mesh neutral alumina is 2:2:1) into the obtained lower layer feed liquid, stirring for 24 hours at normal temperature, and carrying out suction filtration to obtain a filtrate;
4) concentrating the filtrate at 60 deg.C, and drying to obtain ginsenoside extract. Through detection, the content of the total saponins is 72.34%, and the total amount of nicotine and triazole pesticide residues is 48.25 ppm.
Comparative example 2: extracting the ginseng stems and leaves by adopting an extraction method recorded in CN 103550273A:
1) taking 100g of ginseng stem and leaf raw materials, crushing the ginseng stem and leaf raw materials into 40-60 meshes, putting the ginseng stem and leaf raw materials into an extraction tank, adding 1kg of ice water with the temperature of 0 ℃ into the extraction tank, extracting for 10 hours, filtering, collecting filtrate, adding 0.6kg of ice water into filter residues, extracting for the second time, extracting for 10 hours, collecting filtrate, then adding 0.6kg of ice water into the filter residues, extracting for the third time, filtering, collecting filtrate, and combining the three filtrates;
2) vacuum concentrating the above mixed filtrates under reduced pressure to 10 Baume degree under vacuum of-0.1 Mpa at 60 deg.C;
3) adding water saturated n-butanol into the concentrated solution, extracting, separating water phase and n-butanol phase, adding n-butanol into the water phase, separating, extracting, separating two phases, and mixing the n-butanol phases obtained at the previous and subsequent times;
4) vacuum concentrating n-butanol phase under 0.1Mpa at 80 deg.C until no alcohol smell is obtained;
5) adding water into the extract obtained by concentration to prepare extract diluent (the concentrated extract accounts for 10 parts by weight and the water accounts for 90 parts by weight), adding the extract diluent into a pretreated 20g of D101 and DM130 mixed macroporous resin column (the weight ratio of D101 to DM130 is 1:1), and carrying out adsorption at the flow rate of 2BV/h and saturation at the saturation time of 1 h; then washing with distilled water at the washing flow rate of 2BV/h until the effluent is colorless; eluting with 6 times of 70% ethanol solution at the flow rate of 2BV/h, and collecting 70% ethanol eluate;
6) the eluate was concentrated to 8 Baume degree under vacuum (vacuum degree-0.1 Mp) at 60 deg.C, and spray-dried to give the product of comparative example 2. Through detection, the content of the total saponins is 82.20%, and the total amount of nicotine and triazole pesticide residues is 12.1 ppm.
Comparative example 3: extracting the ginseng stems and leaves by adopting an extraction method recorded in CN 1765917A:
taking 100g of ginseng stem and leaf raw materials, crushing and sieving the ginseng stem and leaf raw materials by a 14-mesh sieve, using 15 times of 68% ethanol for cold-soaking extraction at room temperature for 3 times, each time for 13 hours, fully stirring in the extraction process, recovering the solvent from the extracting solution under reduced pressure at 40 ℃, concentrating the extracting solution into an aqueous solution, adding sodium hydroxide into the concentrated solution, adding 3 g of sodium hydroxide into each kilogram of raw materials, enabling the concentration to be 3% and the pH to be 9, putting the sample on a macroporous resin column D101 after all the samples are hydrolyzed under the room temperature condition, washing five column volumes with water, eluting with 70% ethanol to obtain total saponins, recovering the ethanol, and extracting with n-butanol to obtain the panaxadiol group saponins.
Detection shows that the saponin content of the total saponin obtained by the method through 70% ethanol elution is 75.5%, the saponin content of the panaxadiol saponins obtained through n-butanol extraction is 78.5%, and the total content of nicotine and triazole pesticide residues in the two products is 52.8ppm and 24.6ppm respectively.
Compared with the prior art, the extraction method has the advantages that the extraction method has higher total saponin content, obviously reduces the residual quantity of the nicotine and triazole pesticides in the saponin extract, and has excellent technical effect compared with the extraction method in the prior art under the condition of the same raw materials in the example 1 and the comparative examples 1, 2 and 3.
Although the invention has been described in detail hereinabove by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that many modifications and improvements can be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (13)
1.A method for removing nicotine and triazole pesticide residues in total saponins of stems and leaves of saponin plants is characterized in that:
(1) pulverizing saponin plant stems and leaves, adding extraction solvent, extracting, adjusting the pH of the extractive solution to alkalinity, and filtering to obtain filtrate.
(2) Adsorbing the filtrate with macroporous resin column, removing impurities with eluting solvent, washing, discarding, eluting with aqueous ethanol, concentrating the eluate to a certain volume, extracting with organic solvent, discarding the organic layer, adsorbing the water layer with macroporous resin column, eluting with 80-95% ethanol, discarding the eluate, concentrating the lower column solution, and drying to obtain corresponding stem leaf total saponin product.
2. The method according to claim 1, wherein the ground mesh number of the stems and leaves of the saponin plant in the step (1) is 14-80 meshes.
3. The method according to claim 1 or 2, wherein the extraction solvent in step (1) is water or aqueous ethanol.
4. A method according to any one of claims 1 to 3, wherein the extraction solvent in step (1) is aqueous ethanol at a concentration of 50% to 80%.
5. The method according to any one of claims 1 to 4, wherein the extraction solvent in the step (1) is adjusted to a pH of 8 to 13.
6. The method of any one of claims 1 to 5, wherein the pH of the extract of step (1) is adjusted by using KOH or Na2CO3、NaHCO3And one or more of NaOH.
7. The method according to any one of claims 1 to 6, wherein in the step (2), the eluting solvent used for removing impurities is water and aqueous ethanol, and the elution is performed by using water and then using 15 to 35 percent aqueous ethanol.
8. The method according to any one of claims 1 to 7, wherein in step (2), the volume of the elution concentrate is 1/5 to 1/10 times the volume of the starting solution.
9. The method according to any one of claims 1 to 8, wherein in the step (2), the organic solvent used for extraction is one or more of dichloromethane, chloroform, ethyl acetate or n-hexane.
10. The process according to any one of claims 1 to 9, wherein in the step (2), the macroporous resin used for purifying the aqueous layer after extraction is selected from the group consisting of D101, D101C, AB-8, LXPR-2.
11. The stem and leaf total saponin product prepared by the method of any one of claims 1 to 10, which is characterized in that the content of the total saponin is not less than 80%, the nicotine pesticide residue is not more than 0.01ppm, and the triazole pesticide residue is not more than 0.01 ppm.
12. A composition characterized by comprising the stem leaf total saponin product of claim 11.
13. Use of the total stem and leaf saponins or the composition of claims 11 and 12 in the preparation of medicaments for resisting tumors, reducing blood pressure, reducing blood fat, resisting fatigue, improving learning and memory, delaying aging, treating cardiovascular diseases and enhancing immunity.
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